Method for detecting occurrence form of arsenic and mercury in coal
A detection method and morphology technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of time-consuming, laborious, complicated process, inconvenient detection, etc., and achieve the effect of less detection reagents, short detection time and convenient operation
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Embodiment 1
[0030] Guaranteed curve establishment:
[0031] (1) Configuration of methylmercury and inorganic mercury standard solutions: Take 0.485mL methylmercury standard solution and 0.025mL inorganic mercury standard solution respectively in a 25mL volumetric flask, dilute with pure water to make a mixed solution with a concentration of 1 μg / mL Standard solution; then take 0, 0.01, 0.02, 0.04, 0.06, 0.10, 0.20mL of the above solution respectively in a 10mL volumetric flask, dilute with pure water, and prepare the concentrations of 0, 1, 2, 4, 6, 10, 20μg / L series of standard solutions, spare;
[0032] (2) Configuration of trivalent arsenic and pentavalent arsenic standard solutions: take 0.330mL trivalent arsenic standard solution and 1.429mL pentavalent arsenic standard solution respectively in a 25mL volumetric flask, and dilute with pure water to obtain 1 μg / mL standard solution. Mix the solution; then take 0, 0.05, 0.1, 0.2, 0.3, 0.5, 1.0mL of the above solution in a 10mL volumet...
Embodiment 2
[0036] Sample testing:
[0037] Select 1 / 3 coking coal of 6 groups as samples, mark 1-6 groups respectively,
[0038] (1) Treatment of samples to be tested: After collection, each group of samples was dried in an oven at 40°C, then crushed, ground, and passed through a 120-mesh sieve, and the processed samples of each group were stored in paper bags for later use;
[0039] (2) Extraction of arsenic in the sample: Take 0.5g of the above-mentioned treated samples of each group and add 20ml of 0.3mol / L HNO3 to stand overnight, shake and extract at 90°C for 5h, cool to room temperature, centrifuge, and take the supernatant for overnight Put the 0.45μm filter membrane into the bottle to be tested;
[0040] (3) Extraction of mercury in the sample: take 1g of the above-mentioned treated samples of each group and place them in a 50ml centrifuge tube, add 20ml of 6mol / L HCl, extract by shaking at 30°C for 12h, centrifuge, and take 2mL of the supernatant in Add sodium hydroxide solution...
Embodiment 3
[0048] The detection methods such as ICP-MS, AFS, ICP-OES and the detection method of HPLC-AFS of the present invention are compared, and the results are as follows:
[0049] Table 3: Analysis Method Comparison Table
[0050]
[0051] In summary, the present invention has the advantages of high detection efficiency, convenient detection and reduced loss of manpower and material resources.
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